CN104478607A - Thymol bactericide and preparation method thereof - Google Patents
Thymol bactericide and preparation method thereof Download PDFInfo
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- CN104478607A CN104478607A CN201410792481.4A CN201410792481A CN104478607A CN 104478607 A CN104478607 A CN 104478607A CN 201410792481 A CN201410792481 A CN 201410792481A CN 104478607 A CN104478607 A CN 104478607A
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Abstract
The invention discloses a thymol bactericide and a preparation method of several dosage forms of the bactericide. In the thymol bactericide, isopentennyladenine and amino acid are added into thymol so that the thymol bactericide disclosed by the invention can play the bactericidal effect of thymol as well as the plant growth and nutrition promoting effects of isopentennyladenine and amino acid; the indoor bactericidal effects of various dosage forms of the thymol bactericide prove that the bactericidal effect of the thymol bactericide disclosed by the invention is very obvious, and the inhibition rate on mycelial growth is over 80%; and the bactericide has a long lasting period against the diseases such as watermelon powdery mildew, tomato botrytis cinerea, orange acute anthracnose, pepper phytophthora blight and eggplant verticillium wilt while the effect is remarkable. The bactericide is low in toxicity, is environment-friendly, safe and harmless, and has a great market application prospect.
Description
Technical field
The present invention relates to a kind of sterilant, the preparation method of several formulation of the formula of a kind of thymol, isopentennyladenine, amino acid sterilant, and this sterilant specifically.
Background technology
Thymol (Thymol) is the amphyl of cymene, is slightly soluble in water.Its molecular formula is C
10h
14o, chemical name is 2-sec.-propyl-5-methylphenol, and structural formula is:
Thymol because of initial from Thymus vulgaris extraction and isolation out gain the name, it is a kind of semi-transparent clear crystallization, is very easily dissolved in ethanol, ether, acetic acid, chloroform and benzene, has certain fragrance and has very strong germicidal action.On June 19th, 2013, EU Committee has ratified thymol to put on market as plant protection products, and the security of apparent thymol is very high, toxicity is also lower.Thymol also has very wide application such as owing to having antimycotic and parasite function in other side at present, can be used to process wound, makes sanitas, medical bactericide, store dissec etc.; Because it has phenols smell, be also usually used in wormer and spices etc.In addition, thymol also can be used as antioxidant, the qualification special reagent of titanium nitride, the contrast benchmark of thymol blue.Thymol is a kind of active skull cap components, and security is high, is easy to obtain, and stable chemical nature, toxicity is low, easily degrades in the environment, the demand for development of these characteristic conforms biological pesticides.
Isopentennyladenine common name is oxyenadenine+enadenine, it is a class phytokinin, oxyenadenine+enadenine that our doctor's prestige is made through submerged fermentation through the further investigation chain enzyme of more than ten years, being formulated to optimum proportion is 7:1, the bud point growth of plant, tip of a root growth, bud differentiation can be promoted better, fruit tree is increased production.To plant nourish and grow and reproductive growth has the effect of two-ways regulation: when nourishing and growing too vigorous, control to nourish and grow, promote reproductive growth; When reproductive growth is too vigorous, Controlling the procreation growth, promotes to nourish and grow.The cell fission of energy rapid stimulation, alleviates the harm that virus disease causes significantly, prevents early ageing and fruit abscission.And have fine preventive effect function to tomato, cucumber, tobacco virus.
Isopentennyladenine and amino acid is added in thymol, object is the effect that the germicidal action making the present invention can play thymol can play again isopentennyladenine and amino acid whose Promoting plant growth and nutrition, and relevant thymol sterilant, there is not yet relevant report at home and abroad at present.
Thymol sterilant of the present invention, grew and Be very effective disease lasting periods such as watermelon Powdery Mildew, graw mold of tomato, citrus acute anthrax, capsicum epidemic disease, eggplant verticillium wilts.This sterilant low toxicity, environmental protection, safe, harmless, be a kind of sterilant very with market application foreground.
Summary of the invention
The invention provides a kind of thymol sterilant with better fungicidal activity.
The invention provides the aqua, microemulsion, aqueous emulsion, wettable powder, suspended emulsion agent, emulsifiable concentrate, water dispersible granules and preparation method thereof of described thymol sterilant.
Thymol sterilant preferred dosage form of the present invention is aqua and microemulsion.
Thymol sterilization aqua difficulty of the present invention is that thymol is slightly soluble in water, should first thymol synthesis thymol salt, its method is that thymol and potassium hydroxide reaction can generate thymol potassium, then adds isopentennyladenine and thymol sterilization aqua made by other auxiliary agent.
Thymol bactericidal microemulsion of the present invention, can improve drug effect, reduces preparation cost and the usage quantity of organic solvent and the pollution to environment, thus improves agricultural product quality.
Thymol sterilization aqua provided by the present invention, first thymol is made the salt of solubility by above method, make aqua by following composition weight content:
Thymus vulgaris phenates 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 10%,
Amine DA-6 1% ~ 10%,
Stablizer 0.1% ~ 6%,
Surplus is water,
Wherein stablizer is epichlorohydrin, phenyl glycidyl ether, and one or more in cresyl glycidyl ether and polyethylene glycol diglycidylether mix arbitrarily.Water is the one in tap water, distilled water or deionized water.Described stablizer is preferably chloro-1, the 2-propylene oxide of 3-or butylglycidyl ether.The weight percentage of described thymol salt is preferably 10% ~ 20%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 1% ~ 5%.The weight percentage of described stablizer is preferably 0.2% ~ 4%.
Thymol bactericidal microemulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 10%
Amine DA-6 2% ~ 15%,
Solvent 5% ~ 30%,
Emulsifying agent 1% ~ 8%,
Sanitas 1% ~ 8%,
Surplus is water,
Wherein solvent is dimethyl sulfoxide (DMSO), pyrrolidone, and one or more in ethylene glycol, pimelinketone, methyl alcohol and ethanol mix arbitrarily.Emulsifying agent be agriculture breast No. 500, agriculture breast No. 400, agriculture breast No. 1600, agricultural emulsifier NO.600, agriculture breast No. 602 in one or more mix arbitrarily.Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily.Water is the one in tap water, distilled water or deionized water.Described solvent is preferably the one in ethanol or dimethyl sulfoxide (DMSO).The preferred agriculture breast 602 of described emulsifying agent.Described sanitas is preferably the one in nisin or 2-bromo-2-nitro-1,3-propane diol.The weight percentage of described thymol is preferably 10% ~ 20%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 3% ~ 10%.The weight percentage of described solvent is preferably 10% ~ 25%.The weight percentage of described emulsifying agent is preferably 2% ~ 7%.The weight percentage of described sanitas is preferably 1% ~ 5%.
Thymol bactericidal aqueous emulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 12%,
Amine DA-6 1% ~ 12%,
Solvent 5% ~ 30%,
Emulsifying agent 3% ~ 20%,
Sanitas 1% ~ 10%,
Surplus is water,
Wherein solvent is that one or more in dimethyl sulfoxide (DMSO), ethylene glycol, pimelinketone, methyl alcohol and ethanol mix arbitrarily.Emulsifying agent is No. 500, agriculture breast, one or more in No. 400, agriculture breast, No. 1600, agriculture breast, agricultural emulsifier NO.600 number mix arbitrarily.Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily.Water is the one in tap water, distilled water or deionized water.Described solvent is preferably the one in dimethyl sulfoxide (DMSO) or ethanol.Described emulsifying agent is preferably No. 1600, agriculture breast.Described sanitas is preferably nisin.The weight percentage of described thymol is preferably 10% ~ 20%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 1% ~ 5%.The weight percentage of described solvent is preferably 10% ~ 20%.The weight percentage of described emulsifying agent is preferably 5% ~ 8%.The weight percentage of described sanitas is preferably 1% ~ 5%.
Thymol sterilization wettable powder provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 60%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid/11 % ~ 15%,
Amine DA-6 1% ~ 10%,
Carrier 10% ~ 60%,
Dispersion agent 0.2% ~ 5%,
Wetting agent 1% ~ 10%,
Permeate agent 1% ~ 9%,
Wherein carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily.Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily.Wetting agent is that one or more in sodium lauryl sulphate, Witco 1298 Soft Acid, sodium dibutyl naphthalene sulfonate, dioctyl sodium sulfosuccinate mix arbitrarily.Permeate agent be selected from fatty alcohol-polyoxyethylene ether, sulfonated ester, organosilicon one or more mix arbitrarily.Described carrier is preferably kaolin, white carbon black.Described dispersion agent is preferably sodium lignosulfonate.Described wetting agent is preferably Witco 1298 Soft Acid.Described permeate agent is preferably fatty alcohol-polyoxyethylene ether.The weight percentage of described thymol is preferably 20% ~ 45%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 1% ~ 3%.Described carrier is preferably the weight percentage of dispersion agent described in 30% ~ 60%. and is preferably 0.5% ~ 2%.The weight percentage of described wetting agent is preferably 1% ~ 5%.The weight percentage of described permeate agent is preferably 2% ~ 6%.
Thymol bactericidal suspension emulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid/11 % ~ 10%,
Amine DA-6 1% ~ 9%,
Carrier 10% ~ 70%,
Dispersion agent 0.2% ~ 3%,
Emulsifying agent 1% ~ 10%,
Sanitas 1% ~ 12%,
Thickening material 1% ~ 10%,
Defoamer 0.5% ~ 7%,
Surplus is water,
Wherein carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily.Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily.Emulsifying agent is No. 500, agriculture breast, one or more in No. 400, agriculture breast, No. 1600, agriculture breast, No. 600, agriculture breast, Nongru-700 number mix arbitrarily.Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily.Thickening material is that one or more in starch, pectin, agar, gelatin, methylcellulose gum, sodium polyacrylate, white carbon black, Silica hydrogel, carbomer, CMC, polyvinyl ether mix arbitrarily.Defoamer is that one or more in mineral oil, vegetables oil, polyoxyethylene nonylphenol ether, higher alcohols mix arbitrarily.Water is the one in tap water, distilled water or deionized water.Described carrier is preferably kaolin, diatomite.Described dispersion agent is preferably sodium lignosulfonate.Described emulsifying agent is preferably No. 1600, agriculture breast.Described sanitas is preferably nisin.Described thickening material is preferably polyvinyl ether.Described defoamer is preferably mineral oil.The weight percentage of described thymol is preferably 10% ~ 20%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 1% ~ 3%.The weight percentage of described carrier is preferably 10% ~ 50%.The weight percentage of described dispersion agent is preferably 0.5% ~ 2%.The weight percentage of described emulsifying agent is preferably 1% ~ 3%.The weight percentage of described sanitas is preferably 1% ~ 5%.The weight percentage of described thickening material is preferably 1.5% ~ 5%.The weight percentage of described defoamer is preferably 1% ~ 3%.
Thymol sterilization emulsifiable concentrate provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 60%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid 0.5% ~ 10%,
Amine DA-6 1% ~ 12%,
Vegetables oil 20% ~ 80%,
Emulsifying agent 1% ~ 10%,
Wherein emulsifying agent is No. 500, agriculture breast, No. 400, agriculture breast, No. 1600, agriculture breast, one or more in agricultural emulsifier NO.600 mix arbitrarily.Described emulsifying agent is preferably No. 400, agriculture breast, No. 1600, agriculture breast.The weight percentage of described thymol is preferably 10% ~ 30%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 2% ~ 5%.The weight percentage of described vegetables oil is preferably 40% ~ 70%.The weight percentage of described emulsifying agent is preferably 5% ~ 9%.
Thymol sterilized water dispersible granule provided by the present invention, is made up of the component of following weight percent:
Thymol 1% ~ 40%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid 0.2% ~ 10%,
Amine DA-6 1% ~ 10%,
Carrier 40% ~ 85%,
Dispersion agent 0.2% ~ 5%,
Wetting agent 1% ~ 12 %,
Disintegrating agent 0.3% ~ 13%,
Wherein carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily.Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily.Wetting agent is that one or more in sodium lauryl sulphate, Witco 1298 Soft Acid, sodium dibutyl naphthalene sulfonate, dioctyl sodium sulfosuccinate mix arbitrarily.Disintegrating agent is that one or more in dry starch, sodium starch glycolate, low-substituted hydroxypropyl cellulose, croscarmellose sodium mix arbitrarily.Described carrier is preferably kaolin, white carbon black.Described dispersion agent is preferably sodium lignosulfonate.Described wetting agent is preferably Witco 1298 Soft Acid.Described disintegrating agent is preferably dry starch.The weight percentage of described thymol is preferably 10% ~ 30%.The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%.Described amino acid whose weight percentage is preferably 1% ~ 5%.The weight percentage of described amine DA-6 is preferably 3% ~ 5%.The weight percentage of described carrier is preferably 50% ~ 80%.The weight percentage of described dispersion agent is preferably 0.5% ~ 2%.The weight percentage of described wetting agent is preferably 2% ~ 6%.The weight percentage of described disintegrating agent is preferably 1% ~ 5%.
The preparation method of thymol sterilization aqua provided by the present invention is that thymol salt, isopentene gland is fast and amino acid purine is added to the water and dissolves completely, adds amine DA-6, stablizer successively, stirs, be thymol sterilization aqua.
The preparation method of thymol bactericidal microemulsion provided by the present invention, that former for thymol medicine, isopentennyladenine and amino acid solvent are dissolved completely, add amine DA-6, emulsifying agent, sanitas successively, stir, water is added in gained preparation in room temperature high-speed stirring situation, constant temperature stirs evenly, and makes it to form free dispersion, homogeneous, transparent, stable liquid, is thymol bactericidal microemulsion.
The preparation method of thymol bactericidal aqueous emulsion provided by the present invention, that former for thymol medicine, isopentennyladenine and amino acid solvent are dissolved completely, add amine DA-6, emulsifying agent, sanitas successively, stir, water is added in gained preparation in room temperature high-speed stirring situation, constant temperature stirs evenly, and is thymol bactericidal aqueous emulsion.
The preparation method of thymol sterilization wettable powder provided by the present invention, be former for thymol medicine, isopentennyladenine, amino acid, amine DA-6, kaolin, sodium lignosulfonate and fatty alcohol-polyoxyethylene ether are dropped in screw mixer stir, then put into pulverizer and pulverize.Be thymol sterilization wettable powder.
The preparation method of thymol bactericidal suspension emulsion provided by the present invention, that former for thymol medicine, isopentennyladenine, amino acid, kaolin, sodium lignosulfonate, amine DA-6, No. 1600, agriculture breast, nisin, polyvinyl ether, mineral oil are added to the water, porphyrize in sand mill, is thymol bactericidal suspension emulsion.
The preparation method of thymol sterilization emulsifiable concentrate provided by the present invention, be former for thymol medicine is added successively isopentennyladenine, amino acid, amine DA-6, vegetables oil stir, become the transparent liquid of even one, in stirring, add emulsifying agent, be thymol sterilization emulsifiable concentrate.
The preparation method of thymol sterilized water dispersible granule provided by the present invention, former for thymol medicine is added successively in isopentennyladenine, amino acid, amine DA-6, kaolin, sodium lignosulfonate input screw mixer to stir, carry out comminution by gas stream again, carry out high-speed mixing granulation after pulverizing, be thymol sterilized water dispersible granule.
The various formulation of thymol sterilant of the present invention carries out indoor sterilization effect, and its result proves thymol sterilant sterilization effect of the present invention clearly.
Embodiment
The preparation of embodiment 1 thymol potassium
Add 3.755 kilograms of thymols and 2.5l tetrahydrofuran solution in a kettle. until completely dissolved, 1.4 kilograms, potassium hydroxide is added while stirring under cryogenic conditions, react after 2 hours, adjust pH value to neutral with NaHCO3, solvent is removed in the distillation of reactant vacuum decompression, and namely take out reactant is thymol potassium.
The preparation of embodiment 2 thymol sterilization aqua
The preparation of thymol sterilization aqua is made up of the component of following weight percentage:
Thymus vulgaris phenates 18%,
Isopentennyladenine 0.0006%
Amino acid/11 .5%,
Amine DA-6 2%,
Stablizer 1%,
Surplus is water,
Add in 1.8 kilograms of thymol potassium that embodiment 1 obtains, 0.06 gram of isopentennyladenine, 150 grams of amino acid in a kettle. and after 5 kg water are stirred to and dissolve completely, add 100 grams of 3-chloro-1 more successively, 2-propylene oxide, 200 grams of amine DA-6s, add water to gross weight 10 kilograms, stir under normal temperature, namely take out solution from discharge port is thymol sterilization aqua.
Carry out field test with the thymol sterilization aqua in embodiment 2, add in ethanol to make with 18% thymol and compare reagent containing 18% thymol solution.Place: Chengmai, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol sterilization aqua | Mango anthracnose | 1000X | 91.36% | 93.26% | 95.55% |
| Containing 18% thymol solution | Mango anthracnose | 1000X | 60.52% | 65.30% | 67.25% |
The thymol solution sterilization effect that visible thymol sterilization aqua of the present invention compares content is on year-on-year basis obvious, and to mango anthracnose control significantly.
Embodiment 3 thymol bactericidal microemulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 10%,
Isopentennyladenine 0.001%,
Amino acid/11 .2%,
Amine DA-6 6%,
Solvent 20%,
Emulsifying agent 6%,
Sanitas 3%,
Surplus is water,
Add 1 kilogram of former medicine of thymol in a kettle., 0.1 gram of isopentennyladenine, amino acid/11 20 grams, 2 kilograms of ethanol are stirred to and dissolve completely, after add 600 grams of agriculture breasts, 602,600 grams of amine DA-6s, 300 grams of nisins successively, water is added in gained preparation to gross weight 10 kilograms in room temperature high-speed stirring situation, constant temperature stirs evenly, and namely take out reactant after 1 hour is thymol bactericidal microemulsion.
Carry out field test with the thymol bactericidal microemulsion in embodiment 3, add in ethanol to make with 10% thymol and compare reagent containing 10% thymol solution.Place: Chengmai, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol bactericidal microemulsion | Eggplant verticillium wilt | 1000X | 90.52% | 93.26% | 96.55% |
| Containing 10% thymol solution | Eggplant verticillium wilt | 1000X | 50.32% | 55.51% | 57.56% |
The thymol solution sterilization effect that visible thymol bactericidal microemulsion of the present invention compares content is on year-on-year basis obvious, and to the control of tomato early blight significantly.
Embodiment 4 thymol bactericidal aqueous emulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 10%,
Isopentennyladenine 0.001%
Amino acid/11 .5%,
Amine DA-6 2%,
Solvent 18%,
Emulsifying agent 6%,
Sanitas 4%,
Surplus is water,
Add 1 kilogram of former medicine of thymol in a kettle., 0.1 gram of isopentennyladenine, 150 grams of amino acid and 1.8 kilograms of dimethyl sulfoxide (DMSO) are stirred to and dissolve completely, after add 600 grams of agricultures breast No. 1600,200 grams amine DA-6s, 400 grams of nisins successively, add water to gross weight 10 kilograms, constant temperature stirs evenly, and namely the reactant taken out after 1 hour is thymol bactericidal aqueous emulsion.
Carry out field test with the thymol bactericidal aqueous emulsion in embodiment 4, add in ethanol to make with 10% thymol and compare reagent containing 10% thymol solution.Place: Danzhou, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol bactericidal aqueous emulsion | Graw mold of tomato | 1000X | 89.64% | 93.26% | 95.36% |
| Containing 10% thymol solution | Graw mold of tomato | 1000X | 50.02% | 53.26% | 57.22% |
The thymol solution sterilization effect that visible thymol bactericidal aqueous emulsion of the present invention compares content is on year-on-year basis obvious, and remarkable to cucumber downy mildew bacteria-treating.
Embodiment 5 thymol sterilization wettable powder provided by the present invention, is made up of the component of following weight percent:
Thymol 40%,
Isopentennyladenine 0.001%,
Amino acid/11 .2%,
Amine DA-6 2.5%,
Carrier 50%,
Dispersion agent 0.8%,
Wetting agent 2%,
Permeate agent 3%,
Surplus adds carrier to 100%,
Add 4 kilograms of former medicines of thymol in a kettle., 0.1 gram of isopentennyladenine, 120 grams of amino acid, 250 grams of amine DA-6s, 5049.9 grams of kaolin, 80 grams of sodium lignosulfonates, 200 grams of Witco 1298 Soft Acids and 300 grams of fatty alcohol-polyoxyethylene ether high-speed stirring are even, take out reactant after 30 minutes to put into pulverizer and pulverize, sieve.Namely gains are thymol sterilization wettable powders.
Carry out field test with fragrant phenol sterilization wettable powder in embodiment 5, add in ethanol to make with 40% thymol and compare reagent containing 40% thymol solution.Place: Danzhou, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| In fragrant phenol sterilization wettable powder | Watermelon Powdery Mildew | 1000X | 89.53% | 93.17% | 95.31% |
| Containing 40% thymol solution | Watermelon Powdery Mildew | 1000X | 70.62% | 73.27% | 75.12% |
The thymol solution sterilization effect that visible inner fragrant phenol sterilization wettable powder of the present invention compares content is on year-on-year basis obvious, and to powdery mildew of cucumber control significantly.
Embodiment 6 thymol bactericidal suspension emulsion provided by the present invention, is made up of the component of following weight percent:
Thymol 10%,
Isopentennyladenine 0.001%,
Amino acid/11 .5%,
Amine DA-6 2%,
Carrier 20%,
Dispersion agent 1.5%,
Emulsifying agent 2%,
Sanitas 3%,
Thickening material 2.5%,
Defoamer 2%,
Surplus is water,
1 kilogram of former medicine of thymol, 0.1 gram of isopentennyladenine, 150 grams of amino acid, 2 kilograms of kaolin, 150 grams of sodium lignosulfonates, 200 grams of amine DA-6s, 200 grams of agriculture breasts No. 1600,300 grams nisins, 250 grams of polyvinyl ethers, 200 grams of mineral oil are added in 5 kg water, add water to gross weight 10 kilograms, stir, porphyrize in sand mill, namely gains are thymol bactericidal suspension emulsions.
Carry out field test with the thymol bactericidal suspension emulsion in embodiment 6, add in ethanol to make with 10% thymol and compare reagent containing 10% thymol solution.Place: Chengmai, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol bactericidal suspension emulsion | Late blight of tomato | 1000X | 88.30% | 93.25% | 94.21% |
| Containing 10% thymol solution | Late blight of tomato germ | 1000X | 50.02% | 54.24% | 60.21% |
The thymol solution sterilization effect that visible thymol bactericidal suspension emulsion of the present invention compares content is on year-on-year basis obvious, and remarkable to late blight of tomato bacteria-treating.
Embodiment 7 thymol sterilization provided by the present invention emulsifiable concentrate, is made up of the component of following weight percent
Thymol 25%,
Isopentennyladenine 0.001%,
Amino acid 2%,
Amine DA-6 3%,
Vegetables oil 62%,
Emulsifying agent 6%,
Surplus adds vegetables oil and is filled up to 100%,
Stir under adding 2.5 kilograms of former medicines of thymol, 0.1 gram of isopentennyladenine, 200 grams of amino acid, 300 grams of amine DA-6s, 6399.9 grams of vegetables oil normal temperature in a kettle., after 30 minutes, in stirring, add No. 1600,600 grams of agriculture breasts, namely take out reactant after 1 hour is thymol sterilization emulsifiable concentrate.
Carry out field test with the thymol sterilization emulsifiable concentrate in embodiment 7, add in ethanol to make with 25% thymol and compare reagent containing 25% thymol solution.Place: Chengmai, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol sterilization emulsifiable concentrate | Mango anthracnose | 1000X | 83.25% | 87.11% | 91.84% |
| Containing 25% thymol solution | Mango anthracnose | 1000X | 62.24% | 66.29% | 70.23% |
The thymol solution sterilization effect that visible thymol sterilization emulsifiable concentrate of the present invention compares content is on year-on-year basis obvious, and to mango anthracnose control significantly.
Embodiment 8 thymol sterilized water provided by the present invention dispersible granule, is made up of the component of following weight percent:
Thymol 20%,
Isopentennyladenine 0.001%,
Amino acid/11 .9%,
Amine DA-6 3%,
Kaolin 70%,
Dispersion agent 2%,
Wetting agent 2%,
Disintegrating agent 1%,
Surplus kaolin is filled up to 100%,
Add 2 kilograms of former medicines of thymol, 0.1 gram of isopentennyladenine, 190 grams of amino acid, 300 grams of amine DA-6s, 7009.9 grams of kaolin, 200 grams of sodium lignosulfonates, 200 grams of Witco 1298 Soft Acids and 100 grams of dry starch in a kettle., after high-speed stirring is even, carry out comminution by gas stream again, granulation again, obtains thymol sterilized water dispersible granule.
Carry out field test with the thymol sterilized water dispersible granule in embodiment 8, add in ethanol to make with 20% thymol and compare reagent containing 20% thymol solution.Place: Chengmai, Hainan.Experimental result is as following table:
| Reagent agent | Disease | Extension rate | 3d prevention effect | 7d prevention effect | 14d prevention effect |
| Thymol sterilization emulsifiable concentrate | Bacterial blight of rice | 1000X | 80.45% | 85.13% | 92.79% |
| Containing 20% thymol solution | Bacterial blight of rice | 1000X | 60.12% | 64.36% | 72.25% |
The thymol solution sterilization effect that visible thymol sterilized water dispersible granule of the present invention compares content is on year-on-year basis obvious, and to bacterial blight of rice control significantly.And in the field experiment that carries out of the various formulations of above thymol sterilant of the present invention after dispenser plant better than the kindred plant growing way of not dispenser.
Claims (8)
1. thymol sterilization aqua provided by the present invention, first thymol is made the salt of solubility by above method, make aqua by following composition weight content:
Thymus vulgaris phenates 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 10%,
Amine DA-6 1% ~ 10%,
Stablizer 0.1% ~ 6%,
Surplus is water,
It is characterized in that described stablizer is epichlorohydrin, phenyl glycidyl ether, one or more in cresyl glycidyl ether and polyethylene glycol diglycidylether mix arbitrarily; Described stablizer is preferably chloro-1, the 2-propylene oxide of 3-or butylglycidyl ether; Water is the one in tap water, distilled water or deionized water; The weight percentage of described thymol salt is preferably 10% ~ 20%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 1% ~ 5%; The weight percentage of described stablizer is preferably 0.2% ~ 4%; Its preparation method is that thymol salt, isopentene gland is fast and amino acid purine is added to the water and dissolves completely, adds amine DA-6, stablizer successively, stirs, be thymol sterilization aqua.
2. thymol bactericidal microemulsion provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 10%
Amine DA-6 2% ~ 15%,
Solvent 5% ~ 30%,
Emulsifying agent 1% ~ 8%,
Sanitas 1% ~ 8%,
Surplus is water;
It is characterized in that described solvent is dimethyl sulfoxide (DMSO), pyrrolidone, one or more in ethylene glycol, pimelinketone, methyl alcohol and ethanol mix arbitrarily; Described solvent is preferably the one in ethanol or dimethyl sulfoxide (DMSO); Emulsifying agent be agriculture breast No. 500, agriculture breast No. 400, agriculture breast No. 1600, agricultural emulsifier NO.600, agriculture breast No. 602 in one or more mix arbitrarily; The preferred agriculture breast 602 of described emulsifying agent; Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily; Described sanitas is preferably the one in nisin or 2-bromo-2-nitro-1,3-propane diol; Water is the one in tap water, distilled water or deionized water; The weight percentage of described thymol is preferably 10% ~ 20%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 3% ~ 10%; The weight percentage of described solvent is preferably 10% ~ 25%; The weight percentage of described emulsifying agent is preferably 2% ~ 7%; The weight percentage of described sanitas is preferably 1% ~ 5%; Its preparation method is dissolved completely former for thymol medicine, isopentennyladenine and amino acid solvent, add amine DA-6, emulsifying agent, sanitas successively, stir, water is added in gained preparation in room temperature high-speed stirring situation, constant temperature stirs evenly, make it to form free dispersion, homogeneous, transparent, stable liquid, be thymol bactericidal microemulsion.
3. thymol bactericidal aqueous emulsion provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%
Amino acid/11 % ~ 12%,
Amine DA-6 1% ~ 12%,
Solvent 5% ~ 30%,
Emulsifying agent 3% ~ 20%,
Sanitas 1% ~ 10%,
Surplus is water
It is characterized in that described solvent is that one or more in dimethyl sulfoxide (DMSO), ethylene glycol, pimelinketone, methyl alcohol and ethanol mix arbitrarily; Described solvent is preferably the one in dimethyl sulfoxide (DMSO) or ethanol; Emulsifying agent is No. 500, agriculture breast, one or more in No. 400, agriculture breast, No. 1600, agriculture breast, agricultural emulsifier NO.600 number mix arbitrarily; Described emulsifying agent is preferably No. 1600, agriculture breast; Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily; Described sanitas is preferably nisin; Water is the one in tap water, distilled water or deionized water; The weight percentage of described thymol is preferably 10% ~ 20%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 1% ~ 5%; The weight percentage of described solvent is preferably 10% ~ 20%; The weight percentage of described emulsifying agent is preferably 5% ~ 8%; The weight percentage of described sanitas is preferably 1% ~ 5%; Its preparation method is dissolved completely former for thymol medicine, isopentennyladenine and amino acid solvent, add amine DA-6, emulsifying agent, sanitas successively, stir, in room temperature high-speed stirring situation, add water in gained preparation, constant temperature stirs evenly, and is thymol bactericidal aqueous emulsion.
4. thymol sterilization wettable powder provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 60%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid/11 % ~ 15%,
Amine DA-6 1% ~ 10%,
Carrier 10% ~ 60%,
Dispersion agent 0.2% ~ 5%,
Wetting agent 1% ~ 10%
Permeate agent 1% ~ 9%
It is characterized in that described carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily; Described carrier is preferably kaolin, white carbon black; Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily; Described dispersion agent is preferably sodium lignosulfonate; Wetting agent is that one or more in sodium lauryl sulphate, Witco 1298 Soft Acid, sodium dibutyl naphthalene sulfonate, dioctyl sodium sulfosuccinate mix arbitrarily; Described wetting agent is preferably Witco 1298 Soft Acid; Permeate agent be selected from fatty alcohol-polyoxyethylene ether, sulfonated ester, organosilicon one or more mix arbitrarily; Described permeate agent is preferably fatty alcohol-polyoxyethylene ether; The weight percentage of described thymol is preferably 20% ~ 45%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 1% ~ 3%; Described carrier is preferably 30% ~ 60%; The weight percentage of described dispersion agent is preferably 0.5% ~ 2%; The weight percentage of described wetting agent is preferably 1% ~ 5%; The weight percentage of described permeate agent is preferably 2% ~ 6%; Its preparation method former for thymol medicine, isopentennyladenine, amino acid, amine DA-6, kaolin, sodium lignosulfonate and fatty alcohol-polyoxyethylene ether is dropped in screw mixer to stir, put into pulverizer again to pulverize, be thymol sterilization wettable powder.
5. thymol bactericidal suspension emulsion provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 30%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid/11 % ~ 10%,
Amine DA-6 1% ~ 9%,
Carrier 10% ~ 70%,
Dispersion agent 0.2% ~ 3%,
Emulsifying agent 1% ~ 10%,
Sanitas 1% ~ 12%,
Thickening material 1% ~ 10%,
Defoamer 0.5% ~ 7%,
Surplus is water
It is characterized in that described carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily; Described carrier is preferably kaolin, diatomite; Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily; Described dispersion agent is preferably sodium lignosulfonate; Emulsifying agent is No. 500, agriculture breast, one or more in No. 400, agriculture breast, No. 1600, agriculture breast, No. 600, agriculture breast, Nongru-700 number mix arbitrarily; Described emulsifying agent is preferably No. 1600, agriculture breast; Sanitas is Sodium Benzoate, potassium sorbate, Sodium dehydroacetate, calcium propionate, sodium Diacetate, Sodium.alpha.-hydroxypropionate, propylparaben, nisin, hydrogen peroxide, one or more in 2-bromo-2-nitro-1,3-propane diol mix arbitrarily; Described sanitas is preferably nisin; Thickening material is that one or more in starch, pectin, agar, gelatin, methylcellulose gum, sodium polyacrylate, white carbon black, Silica hydrogel, carbomer, CMC, polyvinyl ether mix arbitrarily; Described thickening material is preferably polyvinyl ether; Defoamer is that one or more in mineral oil, vegetables oil, polyoxyethylene nonylphenol ether, higher alcohols mix arbitrarily; Described defoamer is preferably mineral oil; Water is the one in tap water, distilled water or deionized water; The weight percentage of described thymol is preferably 10% ~ 20%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 1% ~ 3%; The weight percentage of described carrier is preferably 10% ~ 50%; The weight percentage of described dispersion agent is preferably 0.5% ~ 2%; The weight percentage of described emulsifying agent is preferably 1% ~ 3%; The weight percentage of described sanitas is preferably 1% ~ 5%; The weight percentage of described thickening material is preferably 1.5% ~ 5%; The weight percentage of described defoamer is preferably 1% ~ 3%; Its preparation method is added to the water former for thymol medicine, isopentennyladenine, amino acid, kaolin, sodium lignosulfonate, amine DA-6, No. 1600, agriculture breast, nisin, polyvinyl ether, mineral oil, porphyrize in sand mill, is thymol bactericidal suspension emulsion.
6. thymol sterilization emulsifiable concentrate provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 60%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid 0.5% ~ 10%,
Amine DA-6 1% ~ 12%,
Vegetables oil 20% ~ 80%
Emulsifying agent 1% ~ 10%
It is characterized in that emulsifying agent is No. 500, agriculture breast, No. 400, agriculture breast, No. 1600, agriculture breast, one or more in agricultural emulsifier NO.600 mix arbitrarily; Described emulsifying agent is preferably No. 400, agriculture breast, No. 1600, agriculture breast; The weight percentage of described thymol is preferably 10% ~ 30%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 2% ~ 5%; The weight percentage of described vegetables oil is preferably 40% ~ 70%; The weight percentage of described emulsifying agent is preferably 5% ~ 9%; Its preparation method be former for thymol medicine is added successively isopentennyladenine, amino acid, amine DA-6, vegetables oil stir, become the transparent liquid of even one, in stirring, add emulsifying agent, be thymol sterilization emulsifiable concentrate.
7. thymol sterilized water dispersible granule provided by the present invention, is made up of the component of following weight percent
Thymol 1% ~ 40%,
Isopentennyladenine 0.0001% ~ 0.3%,
Amino acid 0.2% ~ 10%,
Amine DA-6 1% ~ 10%,
Carrier 40% ~ 85%
Dispersion agent 0.2% ~ 5%,
Wetting agent 1% ~ 12 %
Disintegrating agent 0.3% ~ 13%
It is characterized in that described carrier is kaolin, one or more in diatomite, wilkinite, white carbon black, sour calcium mix arbitrarily; Described carrier is preferably kaolin, white carbon black; Dispersion agent is sodium lignosulfonate, one or more in calcium lignin sulphonate, alkylphenol-polyethenoxy base phosphoric acid ester, tripoly phosphate sodium STPP mix arbitrarily; Described dispersion agent is preferably sodium lignosulfonate; Wetting agent is that one or more in sodium lauryl sulphate, Witco 1298 Soft Acid, sodium dibutyl naphthalene sulfonate, dioctyl sodium sulfosuccinate mix arbitrarily; Described wetting agent is preferably Witco 1298 Soft Acid; Disintegrating agent is that one or more in dry starch, sodium starch glycolate, low-substituted hydroxypropyl cellulose, croscarmellose sodium mix arbitrarily; Described disintegrating agent is preferably dry starch; The weight percentage of described thymol is preferably 10% ~ 30%; The weight percentage of described isopentennyladenine is preferably 0.0002% ~ 0.001%; Described amino acid whose weight percentage is preferably 1% ~ 5%; The weight percentage of described amine DA-6 is preferably 3% ~ 5%; The weight percentage of described carrier is preferably 50% ~ 80%; The weight percentage of described dispersion agent is preferably 0.5% ~ 2%; The weight percentage of described wetting agent is preferably 2% ~ 6%; The weight percentage of described disintegrating agent is preferably 1% ~ 5%; Its preparation method is added successively by former for thymol medicine in isopentennyladenine, amino acid, amine DA-6, kaolin, sodium lignosulfonate input screw mixer to stir, carry out comminution by gas stream again, carry out high-speed mixing granulation after pulverizing, be thymol sterilized water dispersible granule.
8. thymol sterilant according to claims 1 to 7, it is characterized in that described thymol sterilant is to watermelon Powdery Mildew, graw mold of tomato, citrus acute anthrax, capsicum epidemic disease, eggplant verticillium wilt, bacterial blight of rice, mango anthracnose, late blight of tomato Be very effective, the lasting period is long.
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| CN105123803A (en) * | 2015-10-26 | 2015-12-09 | 唐睿 | Botanical fungicide containing thymol and kasugamycin |
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| CN110250215A (en) * | 2019-08-05 | 2019-09-20 | 云南中医药大学 | The new application of volatile oil of Herba Eupatorii |
| CN112263571A (en) * | 2020-10-27 | 2021-01-26 | 青岛大学附属医院 | Application of thymol in preparation of medicine for treating fungal keratitis |
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| CN105152771A (en) * | 2015-08-25 | 2015-12-16 | 陕西澄城国绿果农实业有限公司 | High-nutrient apple cultivation liquid, method for preparing same and method for applying high-nutrient apple cultivation liquid |
| CN105123717A (en) * | 2015-10-26 | 2015-12-09 | 唐睿 | Plant growth regulating composition preparation with synergistic function |
| CN105123700A (en) * | 2015-10-26 | 2015-12-09 | 唐睿 | Insecticidal and bactericidal agent with thymol and arecoline and preparation method of insecticidal and bactericidal agent |
| CN105123803A (en) * | 2015-10-26 | 2015-12-09 | 唐睿 | Botanical fungicide containing thymol and kasugamycin |
| CN105123700B (en) * | 2015-10-26 | 2017-06-16 | 海南博士威农用化学有限公司 | A kind of insecticidal bactericide containing Thymol and arecaline and preparation method thereof |
| CN105638648A (en) * | 2016-01-08 | 2016-06-08 | 广州市生物防治站 | Thymol-emamectin benzoate emulsion in water |
| CN105638648B (en) * | 2016-01-08 | 2018-05-18 | 广州市生物防治站 | A kind of Thymol-emamectin-benzoate aqueous emulsion |
| CN107237215A (en) * | 2017-07-28 | 2017-10-10 | 临朐玉龙造纸有限公司 | Fresh-keeping grease proofing food wrapper and preparation method thereof |
| CN107237215B (en) * | 2017-07-28 | 2019-01-22 | 临朐玉龙造纸有限公司 | Fresh-keeping grease proofing food wrapper and preparation method thereof |
| CN110250215A (en) * | 2019-08-05 | 2019-09-20 | 云南中医药大学 | The new application of volatile oil of Herba Eupatorii |
| CN112263571A (en) * | 2020-10-27 | 2021-01-26 | 青岛大学附属医院 | Application of thymol in preparation of medicine for treating fungal keratitis |
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